JPS6238298B2 - - Google Patents

Info

Publication number
JPS6238298B2
JPS6238298B2 JP57180498A JP18049882A JPS6238298B2 JP S6238298 B2 JPS6238298 B2 JP S6238298B2 JP 57180498 A JP57180498 A JP 57180498A JP 18049882 A JP18049882 A JP 18049882A JP S6238298 B2 JPS6238298 B2 JP S6238298B2
Authority
JP
Japan
Prior art keywords
mol
glass
rare earth
resistance
earth oxides
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP57180498A
Other languages
Japanese (ja)
Other versions
JPS5969443A (en
Inventor
Sukeo Makishima
Tatsuya Nagata
Kojiro Shimodaira
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Original Assignee
KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO filed Critical KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Priority to JP57180498A priority Critical patent/JPS5969443A/en
Publication of JPS5969443A publication Critical patent/JPS5969443A/en
Priority to US06/662,832 priority patent/US4530909A/en
Publication of JPS6238298B2 publication Critical patent/JPS6238298B2/ja
Granted legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00Fibre or filament compositions
    • C03C13/001Alkali-resistant fibres
    • C03C13/002Alkali-resistant fibres containing zirconium
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は希土類酸化物、特にイツトリウム酸化
物を含有するアルミノけい酸塩ガラスの製造法に
関する。 シリカとアルミナからなるアルミノけい酸塩ガ
ラスは、耐熱性が高く、機械的性質も良好であ
り、また耐食性、耐風化性の優れたガラスであ
る。しかし、この系のガラスを得るためには非常
に高温を必要とする。 一般の炭化けい素発熱体を使用する電気炉で
は、1550℃程度の温度までが限度であるために、
この系のガラスは一般の電気炉による溶融法では
製造することができなかつた。 一般にアルカリ酸化物、アルカリ土類酸化物を
含有させると、溶融温度が低下し、1550℃程度の
温度で、一般の炭化けい素を発熱体として使用し
た電気炉を使用してガラスを製造することが可能
となる。しかし、アルカリ酸化物、アルカリ土類
酸化物を含有させると、耐熱性、機械的性質、耐
化学性、耐食塩及び耐風化性の諸性質を低下させ
る問題点がある。 本発明者らはさきに、Y2O3を含有させると、
1550℃程度の一般の電気炉を使用してガラスを製
造し得られると共に、得られるガラスは機械的に
優れたものであることを明らかにした。しかし、
分離Y2O3は高価であるため、それだけコスト高
となる。 本発明者らはY2O3を製造する中間精製物であ
るイツトリウムコンセントレートを利用すべく研
究したところ、Y2O3の原鉱石、例えばゼノタイ
ムより精製して得られるイツトリウムコンセント
レートは、数10%のY2O3と、残りはDy2O3
Nd2O3、CeO2、HO2O3、Yb2O3、Sm2O3
La2O3、Gd2O3、Er2O3等の希土類酸化物よりな
つているが、これをY2O3に代え添加使用してア
ルミノけい酸塩ガラスを製造したところ、(1)
Y2O3のほかの他の含有不純物はアルミノけい酸
塩ガラスの特性、特に耐アルカリ性などに悪影響
がない。(2)これを使用すると分離Y2O3を使用し
た場合よりもガラスの溶融点を約50℃低下し得ら
れ、しかもその価格も1/5であるため、安価とな
ることが分つた。この知見に基いて本発明を完成
した。 本発明におけるアルミノけい酸塩ガラスの
SiO2、Al2O3は、SiO230〜60モル%、Al2O320〜
35モル%、Y2O3を主とする希土類酸化物の合計
10〜30モル%の組成割合であることが必要であ
る。 SiO2が30モル%より少ないと溶融温度が高く
なり、1550℃ではガラスが溶融しない。また60モ
ル%を超えると、希土類含有アルミノけい酸塩ガ
ラスの特性が発揮できなくなる。 Al2O3が20モル%より少ないとガラス化せず、
35モル%を超えると溶融温度が高くなり、1550℃
ではガラスが得られない。 Y2O3コンセントレートを原料としたY2O3を主
とする希土類酸化物の合計が10モル%より少ない
と希土類酸化物含有ガラスとしての特性が発揮で
きず、また1550℃の温度ではガラスが溶融できな
い。30モル%を超えると結晶化してしまいガラス
が得られない。 本発明において言うY2O3コンセントレートと
は、Y2O3の原鉱石、例えばゼノタイムを硫酸分
解法またはアルカリ分解法によつて得られる中間
精製物である。アルカリ分解法で示すと、ゼノタ
イムを徐々に400℃の溶融した苛性ソーダに加え
る。反応は発熱反応で反応終了後冷却して反応物
を水で抽出してリン酸ソーダ、過剰のアルカリは
除去される。得られた希土類水酸化物を少量の塩
酸に溶解し、この溶液にしゆう酸を加えて希土し
ゆう酸塩とし、これを900℃で焼成するイツトリ
ウムコンセントレートが得られる。その分析例を
示すと次の通りである。
The present invention relates to a method for producing aluminosilicate glasses containing rare earth oxides, particularly yttrium oxide. Aluminosilicate glass made of silica and alumina has high heat resistance, good mechanical properties, and excellent corrosion resistance and weathering resistance. However, obtaining this type of glass requires extremely high temperatures. Electric furnaces that use general silicon carbide heating elements have a temperature limit of about 1550℃, so
This type of glass could not be manufactured by a general melting method using an electric furnace. Generally, when alkali oxides and alkaline earth oxides are included, the melting temperature decreases, and glass can be manufactured at a temperature of about 1550°C using an electric furnace that uses general silicon carbide as a heating element. becomes possible. However, when alkali oxides and alkaline earth oxides are contained, there is a problem that various properties such as heat resistance, mechanical properties, chemical resistance, corrosion salt resistance, and weathering resistance are deteriorated. The present inventors first found that when Y 2 O 3 is included,
It was revealed that glass can be produced using a general electric furnace at a temperature of about 1550℃, and that the resulting glass has excellent mechanical properties. but,
Since separated Y 2 O 3 is expensive, the cost increases accordingly. The present inventors conducted research to utilize yttrium concentrate, which is an intermediate refined product for producing Y 2 O 3 , and found that yttrium concentrate obtained by refining Y 2 O 3 raw ore, such as xenotime, , several 10% Y 2 O 3 and the rest Dy 2 O 3 ,
Nd 2 O 3 , CeO 2 , HO 2 O 3 , Yb 2 O 3 , Sm 2 O 3 ,
It consists of rare earth oxides such as La 2 O 3 , Gd 2 O 3 , Er 2 O 3 , etc., but when this was added in place of Y 2 O 3 to produce aluminosilicate glass, (1)
Other impurities other than Y 2 O 3 have no negative effect on the properties of the aluminosilicate glass, especially on the alkali resistance. (2) It was found that using this method lowers the melting point of the glass by about 50°C compared to using isolated Y 2 O 3 , and it is also 1/5th the price, making it cheaper. The present invention was completed based on this knowledge. The aluminosilicate glass in the present invention
SiO2 , Al2O3 is SiO2 30~ 60 mol%, Al2O3 20 ~
35 mol%, total of rare earth oxides mainly consisting of Y 2 O 3
It is necessary that the composition ratio be 10 to 30 mol%. If SiO 2 is less than 30 mol%, the melting temperature will be high, and the glass will not melt at 1550°C. Moreover, if it exceeds 60 mol%, the characteristics of the rare earth-containing aluminosilicate glass cannot be exhibited. If Al 2 O 3 is less than 20 mol%, no vitrification occurs,
If it exceeds 35 mol%, the melting temperature will increase to 1550℃
You can't get glass. If the total amount of rare earth oxides mainly consisting of Y 2 O 3 made from Y 2 O 3 concentrate is less than 10 mol%, the properties of the glass containing rare earth oxides cannot be exhibited, and at a temperature of 1550°C, the glass cannot be melted. If it exceeds 30 mol%, crystallization occurs and glass cannot be obtained. The Y 2 O 3 concentrate referred to in the present invention is an intermediate purified product obtained from Y 2 O 3 raw ore, such as xenotime, by a sulfuric acid decomposition method or an alkali decomposition method. In the alkaline decomposition method, xenotime is gradually added to molten caustic soda at 400°C. The reaction is exothermic and after the reaction is completed, it is cooled and the reactants are extracted with water to remove sodium phosphate and excess alkali. The obtained rare earth hydroxide is dissolved in a small amount of hydrochloric acid, oxalic acid is added to this solution to form a rare earth oxalate salt, and this is calcined at 900°C to obtain a yttrium concentrate. An example of the analysis is as follows.

【表】【table】

【表】 すなわち、鉱石中の成分元素のままで分離操作
を行わないで含有しているものである。 前記ガラス組成のほか、必要に応じTiO2
ZrO2をそれぞれ18モル%、8モル%を超えない
量添加してもよい。TiO2の添加は耐化学性、耐
食性、耐風化性を高める作用をするが、18モル%
を超えると結晶化してしまいガラスが得られな
い。 ZrO2の添加は耐化学性、耐食性、耐風化性、
機械的性質、耐熱性を高める作用をするが、8モ
ル%を超えると結晶化してしまいガラスが得られ
ない。 本発明の方法によると、Y2O3を含有するアル
ミノけい酸塩が安価で、且つ溶融温度も低く、一
般の電気炉で溶解し得られ、また得られるガラス
はアルミノけい酸塩ガラスの特性をそのまま保有
する優れた効果を有する。また、得られたガラス
は高弾性率で、耐アルカリ性が高いのでセメント
と複合して使用し得られる。 実施例 1 精製された光学用酸洗い珪砂50モル%、
Al2O325モル%、イツトリウムコンセントレート
中の希土類酸化物の合計25モル%の割合で調合し
たものを白金ルツボに入れ、電気炉中で約1550℃
で3時間溶融した後、アルミニウム板上に流し出
し放冷した。明るい薄褐色の泡のないガラスが得
られた。 2N―NaOH水溶液中、粉末法(JIS#24〜#35
メツシユ)による95℃、10日間の重量減少は6.5
重量%であつた。 またビツカース硬度は830Kgf/mm2であつた。 実施例 2 精製された光学用酸洗い珪砂35モル%、
Al2O325モル%、イツトリウムコンセントレート
中の希土類酸化物合計25モル%、TiO210モル
%、ZrO25モル%の割合で調合したものを、実施
例1と同様にしてガラスを製造した。得られたガ
ラスは明るい薄褐色の泡のないガラスであつた。 2N―NaOH水溶液中で粉末法による95℃、10日
間の重量減少は1.0重量%であつた。 実施例 3 精製された光学用酸洗い珪砂45モル%、
Al2O325モル%、イツトリウムコンセントレート
中の希土類酸化物の合計25モル%、ZrO25モル%
の割合で調合したものを、実施例1と同様にして
ガラスを製造した。得られたガラスは明るい薄褐
色の泡のないガラスであつた。 2N NaOH水溶液中、粉末法による95℃、10日
間の重量減少は5.0重量%であつた。
[Table] In other words, it is the elemental element contained in the ore without any separation operation. In addition to the above glass composition, TiO 2 ,
ZrO 2 may be added in amounts not exceeding 18 mol % and 8 mol %, respectively. Addition of TiO2 has the effect of increasing chemical resistance, corrosion resistance, and weathering resistance, but at 18 mol%
If it exceeds this amount, crystallization will occur and glass will not be obtained. The addition of ZrO2 has chemical resistance, corrosion resistance, weathering resistance,
It acts to improve mechanical properties and heat resistance, but if it exceeds 8 mol%, it will crystallize and no glass will be obtained. According to the method of the present invention, aluminosilicate containing Y 2 O 3 is inexpensive, has a low melting temperature, and can be melted in a general electric furnace, and the resulting glass has the characteristics of aluminosilicate glass. It has an excellent effect of retaining as it is. Furthermore, the obtained glass has a high modulus of elasticity and high alkali resistance, so it can be used in combination with cement. Example 1 Purified optical grade pickled silica sand 50 mol%,
A mixture of 25 mol% Al 2 O 3 and a total of 25 mol% of rare earth oxides in yttrium concentrate was placed in a platinum crucible and heated at approximately 1550°C in an electric furnace.
After melting for 3 hours, it was poured out onto an aluminum plate and allowed to cool. A light tan bubble-free glass was obtained. In 2N-NaOH aqueous solution, powder method (JIS #24 to #35
The weight loss after 10 days at 95°C was 6.5
It was in weight%. Further, the Bitkers hardness was 830 Kgf/mm 2 . Example 2 Purified optical pickling silica sand 35 mol%,
Glass was prepared in the same manner as in Example 1 using a mixture of 25 mol% Al 2 O 3 , 25 mol % total of rare earth oxides in yttrium concentrate, 10 mol % TiO 2 , and 5 mol % ZrO 2 . Manufactured. The resulting glass was a light tan bubble-free glass. The weight loss during 10 days at 95°C using the powder method in a 2N-NaOH aqueous solution was 1.0% by weight. Example 3 Purified optical grade pickled silica sand 45 mol%,
Al 2 O 3 25 mol %, total rare earth oxides in yttrium concentrate 25 mol %, ZrO 2 5 mol %
A glass was prepared in the same manner as in Example 1 using the following proportions. The resulting glass was a light tan bubble-free glass. The weight loss in a 2N NaOH aqueous solution using the powder method at 95°C for 10 days was 5.0% by weight.

Claims (1)

【特許請求の範囲】 1 SiO230〜60モル%、Al2O320〜35モル%に、
Y2O3を主とする希土類酸化物の合計10〜30モル
%を含有させたアルミノけい酸塩ガラスの製造に
際し、Y2O3を主とする希土類酸化物としてイツ
トリウムコンセントレートを使用することを特徴
とするY2O3を含有するアルミノけい酸塩ガラス
の製造法。 2 前記組成のほかTiO218モル%を超えない
量、ZrO2を8モル%を超えない量を添加したも
のである特許請求の範囲第1項記載の製造法。
[Claims] 1 SiO 2 30 to 60 mol%, Al 2 O 3 20 to 35 mol%,
When producing aluminosilicate glass containing a total of 10 to 30 mol% of rare earth oxides mainly consisting of Y 2 O 3 , yttrium concentrate is used as the rare earth oxide mainly consisting of Y 2 O 3 A method for producing aluminosilicate glass containing Y 2 O 3 , characterized in that: 2. The manufacturing method according to claim 1, wherein in addition to the above composition, TiO 2 is added in an amount not exceeding 18 mol % and ZrO 2 is added in an amount not exceeding 8 mol %.
JP57180498A 1982-10-14 1982-10-14 Manufacture of aluminosilicate glass containing y2o3 Granted JPS5969443A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP57180498A JPS5969443A (en) 1982-10-14 1982-10-14 Manufacture of aluminosilicate glass containing y2o3
US06/662,832 US4530909A (en) 1982-10-14 1984-10-19 Aluminosilicate glass containing Y2 O3 concentrate and ZrO2

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57180498A JPS5969443A (en) 1982-10-14 1982-10-14 Manufacture of aluminosilicate glass containing y2o3

Publications (2)

Publication Number Publication Date
JPS5969443A JPS5969443A (en) 1984-04-19
JPS6238298B2 true JPS6238298B2 (en) 1987-08-17

Family

ID=16084288

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57180498A Granted JPS5969443A (en) 1982-10-14 1982-10-14 Manufacture of aluminosilicate glass containing y2o3

Country Status (2)

Country Link
US (1) US4530909A (en)
JP (1) JPS5969443A (en)

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JPS5969443A (en) 1984-04-19
US4530909A (en) 1985-07-23

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